CN114452927B - One-machine two-purpose reaction device for DNT and DNAN synthesis - Google Patents

One-machine two-purpose reaction device for DNT and DNAN synthesis Download PDF

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Publication number
CN114452927B
CN114452927B CN202210105807.6A CN202210105807A CN114452927B CN 114452927 B CN114452927 B CN 114452927B CN 202210105807 A CN202210105807 A CN 202210105807A CN 114452927 B CN114452927 B CN 114452927B
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partition plate
vertical partition
plate
separator
reactor
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CN114452927A (en
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陈丽珍
陈聪
李晓
王建龙
龚磊
肖芸
潘红霞
方克雄
刘强
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Hubei Dongfang Chemical Industry Co ltd
North University of China
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Hubei Dongfang Chemical Industry Co ltd
North University of China
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06—Preparation of nitro compounds
    • C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
    • C07C201/06—Preparation of nitro compounds
    • C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention relates to a one-machine dual-purpose reaction device for DNT and DNAN synthesis, belonging to the technical field of organic synthesis. The device comprises a separator, a reactor and a stirring shaft, wherein the stirring shaft is driven by a driving motor, a lifting cylinder and stirring paddles are arranged on the stirring shaft, the upper part of the lifting cylinder is positioned in the separator, the lower part of the lifting cylinder is positioned in the reactor, the stirring paddles are positioned in the reactor, the separator is divided into an annular inner cylinder part and an annular outer cylinder part by a partition plate, the right partition plate of the annular outer cylinder part is divided into an organic phase chamber and an inorganic phase chamber, and an organic phase discharge port, an inorganic phase discharge port and a homogeneous phase discharge port are arranged on the corresponding separator. The device realizes that two products of DNT and DNAN are synthesized to share one reaction device, only needs to set configuration before use, does not need to replace other synthesis equipment, greatly simplifies synthesis procedures and improves production efficiency.

Description

One-machine two-purpose reaction device for DNT and DNAN synthesis
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a reaction device for organic synthesis, in particular to a one-machine dual-purpose reaction device for DNT and DNAN synthesis.
Background
DNT, dinitrotoluene of formula C 7 H 6 N 2 O 4 The molecular weight is 213.1, is an important precursor for synthesizing TNT explosive, is usually synthesized by nitrifying mononitrotoluene serving as a raw material through a nitro-sulfur mixed acid system, and has the reaction temperature of 65-80 ℃.
DNAN,2, 4-dinitroanisole with molecular formula of C 7 H 6 N 2 O 5 The molecular weight is 198.13, the melting point is 94 ℃, the density is 1.34g cm < -1 >, and the catalyst is usually synthesized by oxyalkylating 2, 4-dinitrochlorobenzene with methanol in sodium hydroxide solution, and the reaction temperature is 50-65 ℃.
The downstream product TNT of DNT is the most important fusion-cast explosive carrier for nearly a hundred years, DNAN is the low-sensitivity fusion-cast explosive carrier which is paid attention to in recent years, flexible production technology of TNT and DNAN is researched and developed, and one production line is used for meeting market demands, so that the production can be rapidly arranged, the product can be rapidly converted, the equipment investment can be reduced, the production and development period can be shortened, the production land room can be saved, and the method has remarkable social and economic significance.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a one-machine dual-purpose reaction device for synthesizing DNT and DNAN based on the characteristics of similar and similar process flow, feeding mode, nitration (oxyalkylation) reaction temperature and the like.
The invention is realized by the following technical scheme:
a one-machine dual-purpose reaction device for DNT and DNAN synthesis comprises a separator and a reactor, wherein the separator is connected and arranged at the top of the reactor;
the top of the separator is provided with a stirring frame, the stirring frame is provided with a driving motor, the output end of the driving motor is provided with a speed reducer, the speed reducer is connected with a stirring shaft, the stirring shaft penetrates through the separator and then stretches into the reactor, a shaft section of the stirring shaft, which is positioned in the reactor, is provided with stirring paddles, a shaft section of the stirring shaft, which is positioned above the stirring paddles, is provided with a lifting cylinder, and the upper part of the lifting cylinder is positioned in the separator and the lower part of the lifting cylinder is positioned in the reactor;
the separator comprises a bottom plate, the periphery of the bottom plate is fixedly provided with a side wall which extends upwards, an inner ring annular vertical partition plate and an outer ring annular vertical partition plate are fixedly arranged on the bottom plate, the inner ring annular vertical partition plate and the outer ring annular vertical partition plate are arranged concentrically, a through hole for a lifting cylinder to pass through is formed in the part, which is positioned in the inner ring annular vertical partition plate, of the bottom plate, the upper part of the lifting cylinder passes through the through hole and is arranged in the inner ring annular vertical partition plate, the inner ring annular vertical partition plate is tightly attached to the wall of the lifting cylinder, the top cylinder opening of the lifting cylinder is higher than the top cylinder opening of the inner ring annular vertical partition plate, and the top cylinder opening of the outer ring annular vertical partition plate is higher than the top cylinder opening of the lifting cylinder; a top plate is sealed and fixed between the top periphery of the side wall and the outer ring annular vertical partition plate, an annular inner cylinder part is formed at the space part between the inner ring annular vertical partition plate and the outer ring annular vertical partition plate, and an annular outer cylinder part is formed at the space part between the outer ring annular vertical partition plate and the side wall; a radial vertical partition plate arranged along the radial direction is fixed between the outer ring annular vertical partition plate and the side wall, two side plate edges of the radial vertical partition plate are respectively and fixedly connected with the outer ring annular vertical partition plate and the side wall, and the top plate edge and the bottom plate edge of the radial vertical partition plate are respectively and fixedly connected with the top plate and the bottom plate; a liquid outlet is formed in the position, close to one side of the radial vertical partition plate, of the bottom of the inner ring annular vertical partition plate, a horizontal partition plate which is arranged in parallel with the bottom plate and the top plate is fixed between the outer ring annular vertical partition plate and the side wall on the other side of the radial vertical partition plate, three side plate edges of the horizontal partition plate are fixedly connected with the outer ring annular vertical partition plate, the radial vertical partition plate and the side wall respectively, a plate weir which extends upwards and is arranged in the radial direction is fixed at the rest side plate edge of the horizontal partition plate, and an overflow seam is reserved between the top plate edge of the plate weir and the top plate; a vertical partition plate of a phase chamber which is arranged along the radial direction is fixed at a position between the plate type weir and the radial vertical partition plate on the horizontal partition plate, two side plate edges of the vertical partition plate of the phase chamber are respectively and fixedly connected with the annular vertical partition plate of the outer ring and the side wall, and the top plate edge and the bottom plate edge of the vertical partition plate of the phase chamber are respectively and fixedly connected with the top plate and the horizontal partition plate; an organic phase chamber is formed in the space part between the plate-type weir and the vertical partition plate of the phase chamber, an inorganic phase chamber is formed in the space part between the vertical partition plate of the phase chamber and the vertical partition plate of the radial direction, a tubular weir which penetrates through the horizontal partition plate and is vertically arranged is fixed on the horizontal partition plate and is positioned between the vertical partition plate of the phase chamber and the vertical partition plate of the radial direction, and the tubular weir is communicated with the inorganic phase chamber and the annular outer cylinder part; the side wall is respectively provided with an organic phase discharge port, an inorganic phase discharge port and a homogeneous phase discharge port, the organic phase discharge port and the inorganic phase discharge port are arranged on the horizontal partition plate and are closely adjacent to each other, the organic phase discharge port is communicated with the organic phase chamber, the inorganic phase discharge port is communicated with the inorganic phase chamber, the homogeneous phase discharge port is arranged below the horizontal partition plate and is closely adjacent to the bottom plate, and the homogeneous phase discharge port is communicated with the annular outer cylinder part;
the reactor comprises a cylinder body, wherein stirring blades on a stirring shaft are positioned in an inner cavity of the cylinder body, a cooling water coil pipe is arranged in the inner cavity of the cylinder body around the stirring blades, and a water inlet and a water outlet of the cooling water coil pipe pass through the separator and are arranged at the outer side of the top of the separator; the top of the cylinder body is provided with a feed inlet communicated with the inner cavity, and the middle position of the bottom is provided with a discharge outlet communicated with the inner cavity; the wall of the barrel is of a sandwich structure, a medium inlet is arranged at the top of the sandwich, a medium outlet is arranged at the bottom of the sandwich, and the sandwich is filled with a medium.
Further, a clean-out pipe which is communicated with the separator and the reactor is arranged on the bottom plate of the separator, and a clean-out valve is arranged on the clean-out pipe; the separator is provided with a reaction liquid circulating pipe, the reaction liquid circulating pipe penetrates through the separator and is arranged up and down, a bottom pipe orifice of the reaction liquid circulating pipe extends into the reactor, a top pipe orifice of the reaction liquid circulating pipe is arranged on the outer side of the top of the separator, and a reaction liquid circulating valve is arranged on the top pipe orifice of the reaction liquid circulating pipe.
Further, the separator is provided with an observation port and a temperature sensor insertion port.
Further, the lifting cylinder adopts a conical structure.
Further, the stirring blade adopts a three-blade propelling type.
Further, the medium filled in the interlayer is hot water.
Further, the separator and reactor are fabricated from dual phase steel 2205 or 2507.
Compared with the prior art, the invention has the following beneficial effects:
1) The device realizes that two products of DNT and DNAN are synthesized to share one reaction device, only needs to set configuration before use, does not need to replace other synthesis equipment, greatly simplifies synthesis procedures and improves production efficiency;
2) The device improves the utilization rate of equipment, reduces the cost of the equipment and shortens the period of production and development;
3) The device is beneficial to flexible manufacture of TNT and DNAN;
4) The device consists of the separator and the reactor, and the structural design of the two parts is scientific and ingenious, the use is convenient and simple, and the maintenance is light, loose and quick.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic view of the overall structure of the device of the present invention.
Fig. 2 is a front view of a separator in the apparatus of the present invention.
Fig. 3 is a top view of a separator in the apparatus of the present invention.
Fig. 4 is a sectional view A-A in fig. 3.
Fig. 5 is a sectional view of B-B in fig. 3.
In the figure: 1-separator, 2-reactor, 3-stirring frame, 4-driving motor, 5-stirring shaft, 6-lifting cylinder, 7-bottom plate, 8-side wall, 9-inner ring annular vertical partition, 10-outer ring annular vertical partition, 11-top plate, 12-annular inner cylinder part, 13-annular outer cylinder part, 14-radial vertical partition, 15-liquid outlet, 16-horizontal partition, 17-plate weir, 18-overflow slit, 19-phase chamber vertical partition, 20-organic phase chamber, 21-inorganic phase chamber, 22-pipe weir, 23-organic phase outlet, 24-inorganic phase outlet, 25-homogeneous phase outlet, 26-cooling water coil, 27-cooling water coil water inlet and outlet, 28-feed inlet, 29-discharge outlet, 30-medium inlet, 31-medium outlet, 32-sandwich, 33-purge tube, 34-reaction liquid circulation tube, 35-observation port, 36-temperature sensor insertion port.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity or position.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
As shown in FIG. 1, the one-machine dual-purpose reaction device for DNT and DNAN synthesis comprises a separator 1 and a reactor 2, wherein the separator 1 is connected and arranged at the top of the reactor 2, and the separator 1 and the reactor 2 are manufactured by adopting dual-phase steel 2205 or 2507.
The top of the separator 1 is provided with a stirring frame 3, the stirring frame 3 is provided with a driving motor 4, the output end of the driving motor 4 is provided with a speed reducer, the speed reducer is connected with a stirring shaft 5, the stirring shaft 5 penetrates through the separator 1 and then stretches into the reactor 2, a shaft section of the stirring shaft 5 positioned in the reactor 2 is provided with stirring blades, the stirring blades rotate along with the stirring shaft 5, the stirring blades adopt three-blade propulsion, and the rotating speed is adjustable in frequency conversion; the lifting cylinder 6 is arranged on the shaft section of the stirring shaft 5 above the stirring blades, the lifting cylinder 6 rotates along with the stirring shaft 5, the lifting cylinder 6 adopts a conical structure, the upper part of the lifting cylinder 6 is positioned in the separator 1, the lower part of the lifting cylinder 6 is positioned in the reactor 2, and the lifting cylinder 6 has the function of lifting and transferring the reaction liquid in the reactor 2 into the separator 1 through autorotation.
As shown in fig. 2 to 5, the separator 1 comprises a bottom plate 7, a side wall 8 extending upwards is fixed on the periphery of the bottom plate 7, an inner ring-shaped vertical partition plate 9 and an outer ring-shaped vertical partition plate 10 are fixed on the bottom plate 7, the inner ring-shaped vertical partition plate 9 and the outer ring-shaped vertical partition plate 10 are concentric, a through hole for a lifting cylinder 6 to pass through is formed in the part, located in the inner ring-shaped vertical partition plate 9, of the bottom plate 7, the upper part of the lifting cylinder 6 passes through the through hole and then is placed in the inner ring-shaped vertical partition plate 9, the inner ring-shaped vertical partition plate 9 is tightly attached to the wall of the lifting cylinder 6, the top cylinder opening of the lifting cylinder 6 is higher than the top cylinder opening of the inner ring-shaped vertical partition plate 9, and the top cylinder opening of the outer ring-shaped vertical partition plate 10 is higher than the top cylinder opening of the lifting cylinder 6; a top plate 11 is sealed and fixed between the top periphery of the side wall 8 and the outer ring annular vertical partition plate 10, an annular inner cylinder part 12 is formed at the space part between the inner ring annular vertical partition plate 9 and the outer ring annular vertical partition plate 10, and an annular outer cylinder part 13 is formed at the space part between the outer ring annular vertical partition plate 10 and the side wall 8; a radial vertical partition plate 14 which is arranged along the radial direction is fixed between the outer ring annular vertical partition plate 10 and the side wall 8, two side plate edges of the radial vertical partition plate 14 are respectively and fixedly connected with the outer ring annular vertical partition plate 10 and the side wall 8, and the top plate edge and the bottom plate edge of the radial vertical partition plate 14 are respectively and fixedly connected with the top plate 11 and the bottom plate 7; a liquid outlet 15 is formed in the position, close to one side of the radial vertical partition plate 14, of the bottom of the inner ring annular vertical partition plate 9, a horizontal partition plate 16 which is arranged in parallel with the bottom plate 7 and the top plate 11 is fixed between the outer ring annular vertical partition plate 10 and the side wall 8 which are positioned on the other side of the radial vertical partition plate 14, three side plate edges of the horizontal partition plate 16 are fixedly connected with the outer ring annular vertical partition plate 10, the radial vertical partition plate 14 and the side wall 8 respectively, a plate-type weir 17 which extends upwards and is arranged in the radial direction is fixed at the rest side plate edge of the horizontal partition plate 16, and an overflow seam 18 is reserved between the top plate edge of the plate-type weir 17 and the top plate 11; a vertical partition plate 19 of a phase chamber which is arranged along the radial direction is fixed on the horizontal partition plate 16 and positioned between the plate weir 17 and the radial vertical partition plate 14, two side plate edges of the vertical partition plate 19 of the phase chamber are respectively and fixedly connected with the annular vertical partition plate 10 of the outer ring and the side wall 8, and the top plate edge and the bottom plate edge of the vertical partition plate 19 of the phase chamber are respectively and fixedly connected with the top plate 11 and the horizontal partition plate 16; the space part between the plate type weir 17 and the vertical partition plate 19 of the phase chamber forms an organic phase chamber 20, the space part between the vertical partition plate 19 of the phase chamber and the vertical partition plate 14 of the radial direction forms an inorganic phase chamber 21, a tubular weir 22 which penetrates through the horizontal partition plate 16 and is vertically arranged is fixed on the horizontal partition plate 16 at the position between the vertical partition plate 19 of the phase chamber and the vertical partition plate 14 of the radial direction, and the tubular weir 22 is communicated with the inorganic phase chamber 21 and the annular outer cylinder part 13; the side wall 8 is respectively provided with an organic phase discharge hole 23, an inorganic phase discharge hole 24 and a homogeneous phase discharge hole 25, the organic phase discharge hole 23 and the inorganic phase discharge hole 24 are arranged on the close to the horizontal partition plate 16, the organic phase discharge hole 23 is communicated with the organic phase chamber 20, the inorganic phase discharge hole 24 is communicated with the inorganic phase chamber 21, the homogeneous phase discharge hole 25 is arranged below the horizontal partition plate 16 and on the close to the bottom plate 7, and the homogeneous phase discharge hole 25 is communicated with the annular outer cylinder part 13.
As shown in fig. 1, the reactor 2 comprises a cylinder, stirring blades on a stirring shaft 5 are positioned in an inner cavity of the cylinder, a cooling water coil 26 is arranged in the inner cavity of the cylinder around the stirring blades, a water inlet and a water outlet 27 of the cooling water coil penetrate through the separator 1 and are arranged on the outer side of the top of the separator 1, and the cooling water coil 26 is used for cooling during DNT synthesis; the top of the cylinder body is provided with a feed port 28 communicated with the inner cavity, and the middle position of the bottom is provided with a discharge port 29 communicated with the inner cavity; the wall of the barrel is of a sandwich structure, a medium inlet 30 is arranged at the top of the sandwich 32, a medium outlet 31 is arranged at the bottom of the sandwich 32, a medium is filled in the sandwich 32, and the medium adopts hot water for the heat preservation effect of DNAN synthesis.
As shown in fig. 1, a bottom plate 7 of the separator 1 is provided with a purge tube 33 for communicating the separator 1 and the reactor 2, the purge tube 33 is provided with a purge valve, and the purge tube 33 has the function of guiding the reaction liquid remaining in the separator 1 into the reactor 2 after the reaction is completed and then finally discharging the reaction liquid from a discharge port 29 of the reactor 2; the separator 1 is provided with a reaction liquid circulating pipe 34, the reaction liquid circulating pipe 34 penetrates through the separator 1 to be arranged up and down, a bottom pipe orifice of the reaction liquid circulating pipe 34 extends into the reactor 2, a top pipe orifice of the reaction liquid circulating pipe 34 is arranged on the outer side of the top of the separator 1 and is provided with a reaction liquid circulating valve, and the reaction liquid circulating pipe 34 has the function of adaptively adjusting the quantity of reaction liquid in the reactor 2; the separator 1 is further provided with an observation port 35 and a temperature sensor insertion port 36.
The working principle of the device of the invention is as follows:
the reaction liquid in the reactor 2 moves upwards along the lifting cylinder 6 under the stirring of the stirring blades, overflows to the annular inner cylinder part 12 of the separator 1 from the top cylinder opening of the lifting cylinder 6, then flows out from the liquid outlet 15 at the bottom of the annular vertical partition plate 9 of the inner ring and enters the annular outer cylinder part 13, and as the side is blocked by the radial vertical partition plate 14, the reaction liquid entering the annular outer cylinder part 13 can only flow along the annular outer cylinder part 13 for one circle and then reaches the other side of the radial vertical partition plate 14; the separator 1 has two functions of separating or not separating reaction liquid, and the function switching is realized through valve configurations on an organic phase discharge port 23, an inorganic phase discharge port 24 and a homogeneous phase discharge port 25; when the reaction liquid consists of an organic phase and an inorganic phase, the weight of the organic phase is light, and the weight of the inorganic phase is heavy, so that the organic phase is positioned on the upper layer of the reaction liquid, and the inorganic phase is positioned on the lower layer of the reaction liquid, in this case, the organic phase and the inorganic phase are separated, at the moment, the valves of the organic phase discharge port 23 and the inorganic phase discharge port 24 are opened, the valve of the homogeneous phase discharge port 25 is closed, and the organic phase positioned on the upper layer in the reaction liquid overflows the plate weir 17, enters the organic phase chamber 20 from the overflow seam 18, and is finally discharged from the organic phase discharge port 23; the inorganic phase in the lower layer of the reaction liquid enters the inorganic phase chamber 21 through the tubular weir 22 under the action of pressure and is finally discharged from the inorganic phase discharge port 24, thereby completing the separation of the organic phase and the inorganic phase; when the reaction liquid is composed of homogeneous phases, the reaction liquid is not required to be separated, at the moment, the valve of the homogeneous phase discharge port 25 is opened, the valves of the organic phase discharge port 23 and the inorganic phase discharge port 24 are closed, and the reaction liquid is finally discharged from the homogeneous phase discharge port 25.
Example 1
DNAN was synthesized by two inventive devices in series: closing valves of an organic phase discharge port 23 and an inorganic phase discharge port 24 of the two devices and opening a valve of a homogeneous phase discharge port 25, and injecting hot water into an interlayer of the reactor 2 of the two devices for preheating and heat preservation; raw materials 2, 4-dinitrochlorobenzene, liquid caustic soda, methanol and the like are put into a high-level tank according to production ration, the raw materials are respectively and continuously added into a reactor 2 of a first invention device according to a set flow rate ratio for synthesis reaction, reaction liquid is continuously discharged from a homogeneous discharge port 25 of a separator 1 and enters a reactor 2 of a second invention device for maturation reaction, and the reaction liquid is continuously discharged from the homogeneous discharge port 25 of the separator 1 and enters a subsequent washing, separating and drying device to finally obtain a refined product. The purity of the discharged material of the first device is 94.2%, the purity of the discharged material of the second device is 98.6%, the melting point of the final product is 96 ℃, and the yield is 99.1%.
Example 2
DNT was synthesized by two inventive apparatus connected in series: the valves of the organic phase discharge port 23 and the inorganic phase discharge port 24 of the device are opened, the valves of the homogeneous phase discharge port 25 are closed, and cooling water is injected into the cooling water coil 26 for cooling during DNT synthesis; adding raw materials of mononitrotoluene, 98% concentrated sulfuric acid, 98% concentrated nitric acid and the like into a high-level tank according to production quota, respectively and continuously adding the raw materials into a reactor 2 of a first invention device and a reactor 2 of a second invention device according to a set flow rate ratio for synthesis reaction, continuously discharging an upper material of a reaction liquid in the first invention device from an organic phase discharge port 23 of the reactor 2 and entering the reactor 2 of the second invention device for further reaction, continuously discharging a lower material of the reaction liquid in the first invention device from an inorganic phase discharge port 24 of the reactor 2 and entering a special receiving device; the lower material of the reaction liquid in the device of the second invention is continuously discharged from the inorganic phase discharge port 24 of the reactor 2 and enters the reactor 2 of the device of the first invention, and the upper material is continuously discharged from the organic phase discharge port 23 of the reactor 2 and enters a subsequent washing, separating and drying device, so that the refined product is finally obtained. The purity of the discharged material of the second device is 97.4%, the melting point of the product is 48-51 ℃, and the yield is 99.3%.
The foregoing has been a clear and complete description of the technical solutions of embodiments of the present invention, and the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (7)

1. A one-machine-two-purpose reaction device for synthesizing DNT and DNAN, which is characterized in that: the device comprises a separator and a reactor, wherein the separator is connected and arranged at the top of the reactor;
the top of the separator is provided with a stirring frame, the stirring frame is provided with a driving motor, the output end of the driving motor is provided with a speed reducer, the speed reducer is connected with a stirring shaft, the stirring shaft penetrates through the separator and then stretches into the reactor, a shaft section of the stirring shaft, which is positioned in the reactor, is provided with stirring paddles, a shaft section of the stirring shaft, which is positioned above the stirring paddles, is provided with a lifting cylinder, and the upper part of the lifting cylinder is positioned in the separator and the lower part of the lifting cylinder is positioned in the reactor;
the separator comprises a bottom plate, the periphery of the bottom plate is fixedly provided with a side wall which extends upwards, an inner ring annular vertical partition plate and an outer ring annular vertical partition plate are fixedly arranged on the bottom plate, the inner ring annular vertical partition plate and the outer ring annular vertical partition plate are arranged concentrically, a through hole for a lifting cylinder to pass through is formed in the part, which is positioned in the inner ring annular vertical partition plate, of the bottom plate, the upper part of the lifting cylinder passes through the through hole and is arranged in the inner ring annular vertical partition plate, the inner ring annular vertical partition plate is tightly attached to the wall of the lifting cylinder, the top cylinder opening of the lifting cylinder is higher than the top cylinder opening of the inner ring annular vertical partition plate, and the top cylinder opening of the outer ring annular vertical partition plate is higher than the top cylinder opening of the lifting cylinder; a top plate is sealed and fixed between the top periphery of the side wall and the outer ring annular vertical partition plate, an annular inner cylinder part is formed at the space part between the inner ring annular vertical partition plate and the outer ring annular vertical partition plate, and an annular outer cylinder part is formed at the space part between the outer ring annular vertical partition plate and the side wall; a radial vertical partition plate arranged along the radial direction is fixed between the outer ring annular vertical partition plate and the side wall, two side plate edges of the radial vertical partition plate are respectively and fixedly connected with the outer ring annular vertical partition plate and the side wall, and the top plate edge and the bottom plate edge of the radial vertical partition plate are respectively and fixedly connected with the top plate and the bottom plate; a liquid outlet is formed in the position, close to one side of the radial vertical partition plate, of the bottom of the inner ring annular vertical partition plate, a horizontal partition plate which is arranged in parallel with the bottom plate and the top plate is fixed between the outer ring annular vertical partition plate and the side wall on the other side of the radial vertical partition plate, three side plate edges of the horizontal partition plate are fixedly connected with the outer ring annular vertical partition plate, the radial vertical partition plate and the side wall respectively, a plate weir which extends upwards and is arranged in the radial direction is fixed at the rest side plate edge of the horizontal partition plate, and an overflow seam is reserved between the top plate edge of the plate weir and the top plate; a vertical partition plate of a phase chamber which is arranged along the radial direction is fixed at a position between the plate type weir and the radial vertical partition plate on the horizontal partition plate, two side plate edges of the vertical partition plate of the phase chamber are respectively and fixedly connected with the annular vertical partition plate of the outer ring and the side wall, and the top plate edge and the bottom plate edge of the vertical partition plate of the phase chamber are respectively and fixedly connected with the top plate and the horizontal partition plate; an organic phase chamber is formed in the space part between the plate-type weir and the vertical partition plate of the phase chamber, an inorganic phase chamber is formed in the space part between the vertical partition plate of the phase chamber and the vertical partition plate of the radial direction, a tubular weir which penetrates through the horizontal partition plate and is vertically arranged is fixed on the horizontal partition plate and is positioned between the vertical partition plate of the phase chamber and the vertical partition plate of the radial direction, and the tubular weir is communicated with the inorganic phase chamber and the annular outer cylinder part; the side wall is respectively provided with an organic phase discharge port, an inorganic phase discharge port and a homogeneous phase discharge port, the organic phase discharge port and the inorganic phase discharge port are arranged on the horizontal partition plate and are closely adjacent to each other, the organic phase discharge port is communicated with the organic phase chamber, the inorganic phase discharge port is communicated with the inorganic phase chamber, the homogeneous phase discharge port is arranged below the horizontal partition plate and is closely adjacent to the bottom plate, and the homogeneous phase discharge port is communicated with the annular outer cylinder part;
the reactor comprises a cylinder body, wherein stirring blades on a stirring shaft are positioned in an inner cavity of the cylinder body, a cooling water coil pipe is arranged in the inner cavity of the cylinder body around the stirring blades, and a water inlet and a water outlet of the cooling water coil pipe pass through the separator and are arranged at the outer side of the top of the separator; the top of the cylinder body is provided with a feed inlet communicated with the inner cavity, and the middle position of the bottom is provided with a discharge outlet communicated with the inner cavity; the wall of the barrel is of a sandwich structure, a medium inlet is arranged at the top of the sandwich, a medium outlet is arranged at the bottom of the sandwich, and the sandwich is filled with a medium.
2. The one-machine dual-purpose reaction device for DNT and DNAN synthesis according to claim 1, wherein: a clean-out pipe which is communicated with the separator and the reactor is arranged on the bottom plate of the separator, and a clean-out valve is arranged on the clean-out pipe; the separator is provided with a reaction liquid circulating pipe, the reaction liquid circulating pipe penetrates through the separator and is arranged up and down, a bottom pipe orifice of the reaction liquid circulating pipe extends into the reactor, a top pipe orifice of the reaction liquid circulating pipe is arranged on the outer side of the top of the separator, and a reaction liquid circulating valve is arranged on the top pipe orifice of the reaction liquid circulating pipe.
3. The one-machine dual-purpose reaction device for DNT and DNAN synthesis according to claim 2, wherein: the separator is provided with an observation port and a temperature sensor insertion port.
4. A one-machine dual-purpose reaction device for DNT and DNAN synthesis according to any of claims 1-3, characterized in that: the lifting cylinder adopts a conical structure.
5. The one-machine-dual-purpose reaction device for DNT and DNAN synthesis according to claim 4, wherein: the stirring blade adopts three-blade propulsion.
6. A one-machine dual-purpose reaction device for DNT and DNAN synthesis according to any of claims 1-3, characterized in that: the medium filled in the interlayer is hot water.
7. A one-machine dual-purpose reaction device for DNT and DNAN synthesis according to any of claims 1-3, characterized in that: the separator and reactor are fabricated from dual phase steel 2205 or 2507.
CN202210105807.6A 2022-01-28 2022-01-28 One-machine two-purpose reaction device for DNT and DNAN synthesis Active CN114452927B (en)

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Publication number Priority date Publication date Assignee Title
KR20030019191A (en) * 2001-08-30 2003-03-06 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 Monolith catalytic reactor coupled to static mixer
CN113121356A (en) * 2021-03-23 2021-07-16 中化安全科学研究(沈阳)有限公司 Automatic power continuous nitration method and device

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030019191A (en) * 2001-08-30 2003-03-06 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 Monolith catalytic reactor coupled to static mixer
CN113121356A (en) * 2021-03-23 2021-07-16 中化安全科学研究(沈阳)有限公司 Automatic power continuous nitration method and device

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